The alcohols R.sub.f CH.sub.2 CH.sub.2 OH are valuable intermediates for preparing oil and water repellants, surface active agents, lubricants and a number of other useful materials. A previously disclosed method for the preparation of those alcohols consists of two reactions carried out in sequence. The first is the reaction of the iodide, R.sub.f CH.sub.2 CH.sub.2 I, with oleum to form the polyfluoroalkyl hydrogen sulfate ester, R.sub.f CH.sub.2 CH.sub.2 OSO.sub.2 OH, and I.sub.2. The second is the hydrolysis of the ester, R.sub.f CH.sub.2 CH.sub.2 OSO.sub.2 OH, with aqueous acid to the alcohol, R.sub.f CH.sub.2 CH.sub.2 OH, and sulfuric acid; see U.S. Pat. No. 3,283,012. While the foregoing method has been used in the industry for some years, it is not without its drawbacks. The 2-perfluoroalkylethanols contain small amounts of R.sub.f CH.sub.2 CH.sub.2 I and R.sub.f I. If those iodides are not removed or converted, discolored products result and corrosive HF is produced. In the past, the 2-perfluoroalkylethanols have been purified by heating them in the presence of small amounts of hydrogen peroxide, thereby oxidizing the iodide to the organic acid, HF and iodine. The resulting waste products are then removed by a sodium bisulfite wash followed by washing with dilute aqueous phosphoric acid.